Anhydrous perchloric acid is not stable and sulfuric acid will not help to stabilize it. I would expect such a mixture to explode within minutes if not immediately. This procedure is not the same as making perchloric acid in acetic acid for use as a non-aqueous titrant. In that solution, the perchlorate is still in the form of a dihydrate so is stable. Sulfuric acid and oleum are strong dehydrating agents that will remove the water of hydration from perchloric acid, making it unstable.
GFS Chemicals has a long history of making perchloric acid and perchlorate salts. In the past, we made anhydrous perchlorate as a raw material that was consumed shortly after being made. We stopped that practice more than 30 years ago. I forwarded this email to our retired chief chemist for his comments. He actually worked with anhydrous perchloric acid during his tenure here. While I wait for his response I felt compelled to send this warning.
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Does anyone know of a potential hazard of mixing 70% perchloric acid with oleum (% SO3 to react with most of the water in the perchloric acid).
The research group is trying to make ~100% sulfuric acid and ~100% perchloric acid to oxidize small quanities of carbon (graphite) at temperatures ranging up to 70 C. The group understands the usual problems with handling oleum and they know that 100% perchloric acid by its self is a major safety problem.
Concentrations of the "100% perchloric acid" would be in the range of 10 to 30% in the oleum.
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